反应详情

温度

100 °C

2-(7-(2-methoxyethoxy)-[1,2,4]triazolo[4,3-a]pyridin-3-yl)quinolin-8-yl trifluoromethane sulfonate (0.027 g, 0.0576 mmol), tert-butyl piperazine-1-carboxylate (0.0215 g, 0.115 mmol), Cs2CO3 (0.0282 g, 0.0865 mmol), Pd2dba3 (0.00528 g, 0.00576 mmol) and Binap-rac (0.00718 g, 0.0115 mmol) were combined in toluene (0.5 mL) in a sealed vial. The reaction mixture was stirred at 100° C. for 16 hours then concentrated under reduced pressure. The resulting residue was diluted with EtOAc, washed with aqueous saturated NaHCO3 and brine, dried over Na2SO4, filtered and concentrated under reduced pressure to an orange solid. Purification via flash column chromatography (40:1 DCM/MeOH followed by 20:1 DCM/MeOH) provided 22 mg (76%) of desired product.

1. concentrationthen concentrated under reduced pressure
2. additionThe resulting residue was diluted with EtOAc
3. washwashed with aqueous saturated NaHCO3 and brine
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure to an orange solid
7. customPurification via flash column chromatography (40:1 DCM/MeOH followed by 20:1 DCM/MeOH)